CN102432972A - Method for preparing nano composite hydrogel with magnetic function - Google Patents
Method for preparing nano composite hydrogel with magnetic function Download PDFInfo
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- CN102432972A CN102432972A CN2011103011038A CN201110301103A CN102432972A CN 102432972 A CN102432972 A CN 102432972A CN 2011103011038 A CN2011103011038 A CN 2011103011038A CN 201110301103 A CN201110301103 A CN 201110301103A CN 102432972 A CN102432972 A CN 102432972A
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Abstract
The invention relates to a method for preparing nano composite hydrogel with magnetic function. The method comprises the following steps of: (1) adding inorganic clay into deionized water, stirring to completely strip the clay, adding a water-soluble monomer, an initiator and a catalyst, mixing uniformly to obtain a prepolymer solution, and polymerizing the obtained prepolymer solution at the temperature of between 5 and 30 DEG C for 24 to 120 hours to obtain nano composite hydrogel; and (2) dissolving a bivalent iron salt and a trivalent iron salt into deionized water, adding 1 to 10 grams of the nano composite hydrogel, soaking for 24 to 120 hours at the temperature of between 5 and 30 DEG C under the protection of nitrogen to obtain soaked hydrogel, preparing 0.5 to 5mol/L co-precipitator, adding the soaked hydrogel, reacting for 1 to 12 hours under the protection of nitrogen, and thus obtaining the nano composite hydrogel with magnetic function. The preparing method is simple, wide in raw material source and low in cost; and the obtained nano composite hydrogel has excellent magnetic performance and high application value.
Description
Technical field
The invention belongs to the preparation field of Nanometer composite hydrogel, particularly a kind of preparation method with Nanometer composite hydrogel of magnetic function.
Background technology
The multicomponent system that macromolecule hydrogel is made up of polymer three-dimensional network and aqueous solvent can cause behind the absorption large quantity of moisture that the macroscopic view of polymer network changes.Hydrogel has solid on macroscopic view can not mobile character, and the behavior that is similar to solution is arranged on microcosmic, can be in water swelling, but do not dissolve.Although the water in the hydrogel is bound by in the gel network, still have certain reactivity, this structure that is similar to organism has excellent biological compatibility.The organic/inorganic nano composite aquogel is in three-dimensional network, to introduce the nano grade inorganic clay as the physical crosslinking point, forms three-dimensional net structure through the non covalent bond effect between the molecular chain.
In recent years; Patent report is arranged, and (like publication number is CN101531742A; CN101215350A) be linking agent with commercially available inorganic lithium saponite (Laponite XLG, Laponite XLS); Utilize the physical crosslinking effect (hydrogen bond, hydrophobic force, Coulomb force, electrostatic adhesion or physical entanglement) between polymer molecular chain and the clay; Original position has been synthesized clay/polymer nanocomposite composite aquogel, has greatly improved mechanical property, water absorbing properties, the optical transmission of gel, has widened the application of gel aspect chemical machinery, high-absorbent material.
Yet; Also there is certain defective in this hydrogel material aspect functional the constructing (temperature, pH, light, electricity, magnetic responsiveness); Through constructing intelligent gel with certain responsiveness; With make gel to external world environment response more rapidly, intelligent response property is more comprehensive, further expands the application of gel in fields such as chemical machinery, biomedicine and organizational projects.Realize hydrogel intelligent response property and strong mechanical performance to combine be the main trend of following gel development.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method with Nanometer composite hydrogel of magnetic function; This method technology is simple; Cost is lower, and the magnetic Nano composite aquogel that obtains has excellent magnetic response performance, and the material choice scope of this method is big in addition; Overcome functional single, the magnetic response defect of insufficient of common Nanometer composite hydrogel, have higher using value.
A kind of preparation method with Nanometer composite hydrogel of magnetic function of the present invention comprises:
(1) preparation of Nanometer composite hydrogel:
Inorganic clay is joined in the deionized water, clay is peeled off fully, add water-soluble monomer, initiator, catalyzer then, obtain pre-polymerization liquid after mixing; The pre-polymerization liquid of gained at 5-30 ℃ of following polymerization 24-120 hour, is obtained Nanometer composite hydrogel; Wherein the massfraction of pre-polymerization liquid medium clay soil is 0.1%-20%, and the massfraction 5%-40% of water-soluble monomer, the massfraction of initiator are 0.5%-2%, and the massfraction of catalyzer is 0.0001%-0.01%, and all the other compositions are deionized water;
(2) magnetic of Nanometer composite hydrogel is constructed:
Be dissolved in divalent iron salt and trivalent iron salt in the deionized water, add the above-mentioned Nanometer composite hydrogel of 1g-10g again, under 5-30 ℃ and nitrogen protection, soaked 24-120 hour the hydrogel after obtaining soaking;
Configuration 0.5-5mol/L coprecipitator adds the hydrogel after the above-mentioned immersion, and nitrogen protection reaction 1-12 hour down promptly gets the Nanometer composite hydrogel with magnetic function; The mol ratio of raw material is a divalent iron salt: trivalent iron salt: coprecipitator=1: 1-2.5: 1-20.
Inorganic clay in the said step (1) is meant the inorganic lithium saponite that in water, can peel off fully, is Laponite XLG or Laponite XLS (commercially available), and wherein the chemical formula of Laponite XLG is [Mg
5.34Li
0.66Si
8O
20(OH)
4] Na
0.66, Laponite XLS is 92.32% [Mg by massfraction
5.34Li
0.66Si
8O
20(OH)]
4] Na
0.66With massfraction be 7.68% Na
4P
2O
7Form.
Water-soluble monomer in the said step (1) is one or more in NSC 11448, vinylformic acid, the acrylic amide.
Initiator in the said step (1) is one or more in Potassium Persulphate, ammonium persulphate, Sodium Persulfate, the Diisopropyl azodicarboxylate.
Catalyzer in the said step (1) is N, N, N ', N ', one or more in-Tetramethyl Ethylene Diamine, trolamine, the Sulfothiorine.
Divalent iron salt in the said step (2) is FeSO
47H
2O, FeSO
4, FeCl
2, FeCl
24H
2Among the O one or more.
Ferric salt solution in the said step (2) is Fe
2(SO
4)
3, Fe
2(SO
4)
39H
2O, FeCl
3, FeCl
36H
2Among the O one or more.
Coprecipitator in the said step (2) is one or more in sodium hydroxide solution, potassium hydroxide solution, the ammoniacal liquor.
The saturation magnetization of the Nanometer composite hydrogel with magnetic function that obtains in the said step (2) is between 0.5-30emu/g, and coercive force is between 0-50Oe.
The particle diameter of magnetic nanoparticle is between 10-100nm in the Nanometer composite hydrogel with magnetic function that obtains in the said step (2), and the massfraction of magnetic nanoparticle accounts for the 1%-30% of the hydrogel with magnetic function.
The Nanometer composite hydrogel with magnetic function that obtains in the said step (2) can have magnetic responsiveness, temperature-responsive and pH responsiveness.
The present invention utilizes the adsorption of divalence and ferric ion and gel network and molecular chain, in organic/inorganic nano composite aquogel matrix, successfully constructs magnetic function, has realized the magnetic response of hydrogel material.Preparation with Nanometer composite hydrogel of magnetic function is characterized in that Z 250 is introduced in the three-dimensional network of Nanometer composite hydrogel; Magnetic particle is uniformly dispersed; Particle diameter is between 10-100nm; The saturation magnetization of this gel is between 0.5-30emu/g, and coercive force is between 0-50Oe.
Beneficial effect
(1) the present invention generates magnetic nano-particle through chemical coprecipitation original position in the Nanometer composite hydrogel three-dimensional network, and this method technology is simple, and raw material sources are extensive, and cost is lower, applicable to batch process;
(2) the magnetic Nano composite aquogel of the present invention's preparation has fixed shape, and saturation magnetization is adjustable, satisfactory stability property and intelligent response property; Nanometer composite hydrogel from now on functional constructed important reference.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
(1) in the 30g deionized water, add 1.5g inorganic clay Laponite XLS, after fully stirring with the 6.39g acrylic amide, the 0.06g Potassium Persulphate; 0.01gN, N, N '; N ' ,-Tetramethyl Ethylene Diamine join in the aqueous solution of clay and obtain transparent pre-polymerization liquid, then pre-polymerization liquid are injected into long 40mm; Diameter is in the Glass tubing of 6mm, obtains Nanometer composite hydrogel in 48 hours 25 ℃ of following polymerizations.
(2) with 10gFeCl
24H
2O and 20gFeCl
36H
2O is dissolved in the 100g deionized water fully, and to wherein leading to N
230min is to remove O residual in the solution
2, add the 5g Nanometer composite hydrogel, soaked 24 hours down at 25 ℃.Configuration 1mol/L sodium hydroxide solution 100mL puts into the gel after the immersion, and reaction is 5 hours in closed reactor, and whole process is at N
2Carry out in the atmosphere, preparation has the Nanometer composite hydrogel of magnetic function.
Embodiment 2
(1) in the 30g deionized water, adds 4.5g inorganic clay Laponite XLS; After fully stirring with the 10.65g acrylic amide; 0.1g Potassium Persulphate, 0.01g Diisopropyl azodicarboxylate join in the aqueous solution of clay and obtain transparent pre-polymerization liquid, then pre-polymerization liquid are injected into long 40mm; Diameter is in the Glass tubing of 6mm, obtains Nanometer composite hydrogel in 24 hours 25 ℃ of following polymerizations.
(2) with 10gFeCl
24H
2O and 20gFeCl
36H
2O is dissolved in the 100g deionized water fully, and to wherein leading to N
230min is to remove O residual in the solution
2, add the 5g Nanometer composite hydrogel, soaked 48 hours down at 25 ℃.Configuration 1mol/L sodium hydroxide solution 100mL puts into the gel after the immersion, and reaction is 5 hours in closed reactor, and whole process is at N
2Carry out in the atmosphere, preparation has the Nanometer composite hydrogel of magnetic function.
Embodiment 3
(1) in the 30g deionized water, adds 0.15g inorganic clay Laponite XLG; After fully stirring with the 2.13g acrylic amide; 0.02g ammonium persulphate, 0.01g trolamine join in the aqueous solution of clay and obtain transparent pre-polymerization liquid, then pre-polymerization liquid are injected into long 40mm; Diameter is in the Glass tubing of 6mm, obtains Nanometer composite hydrogel in 96 hours 25 ℃ of following polymerizations.
(2) with 5gFeCl
24H
2O and 10gFeCl
36H
2O is dissolved in the 100g deionized water fully, and to wherein leading to N
230min is to remove O residual in the solution
2, add the 5g Nanometer composite hydrogel, soaked 24 hours down at 25 ℃.Whole process is at N
2Carry out in the atmosphere, configuration 1mol/L sodium hydroxide solution 100mL puts into the gel after the immersion, and reaction is 2 hours in closed reactor, and preparation has the Nanometer composite hydrogel of magnetic function.
Embodiment 4
(1) in the 30g deionized water, adds 1.5g inorganic clay Laponite XLS; After fully stirring with the 3.39g NSC 11448; 0.03g ammonium persulphate, 0.01g trolamine join in the aqueous solution of clay and obtain transparent pre-polymerization liquid, then pre-polymerization liquid are injected into long 40mm; Diameter is in the Glass tubing of 6mm, obtains Nanometer composite hydrogel in 48 hours 25 ℃ of following polymerizations.
(2) with 6.4gFeCl
2And 12.3gFeCl
3Be dissolved in fully in the 100g deionized water, and to wherein leading to N
230min is to remove O residual in the solution
2, add the 5g Nanometer composite hydrogel, soaked 24 hours down at 25 ℃.Configuration 10mol/L ammoniacal liquor 100mL puts into the gel after the immersion, and reaction is 12 hours in closed reactor, and whole process is at N
2Carry out in the atmosphere, preparation has the Nanometer composite hydrogel of magnetic function.
Embodiment 5
(1) in the 30g deionized water, add 2.4g inorganic clay Laponite XLS, after fully stirring with the 3.39g NSC 11448, the 0.06g Potassium Persulphate; 0.01gN, N, N '; N ' ,-Tetramethyl Ethylene Diamine join in the aqueous solution of clay and obtain transparent pre-polymerization liquid, then pre-polymerization liquid are injected into long 40mm; Diameter is in the Glass tubing of 6mm, obtains Nanometer composite hydrogel in 48 hours 25 ℃ of following polymerizations.
(2) with 14gFeSO
47H
2O and 32gFe
2(SO
4)
39H
2O is dissolved in the 100g deionized water fully, and to wherein leading to N
230min is to remove O residual in the solution
2, add the 10g Nanometer composite hydrogel, soaked 120 hours down at 25 ℃.Configuration 1mol/L potassium hydroxide solution 100mL puts into the gel after the immersion, and reaction is 12 hours in closed reactor, and whole process is at N
2Carry out in the atmosphere, preparation has the Nanometer composite hydrogel of magnetic function.
Embodiment 6
(1) in the 50g deionized water, add 1g inorganic clay Laponite XLG, after fully stirring with the 11.3g NSC 11448, the 0.1g Potassium Persulphate; 0.01gN, N, N '; N ' ,-Tetramethyl Ethylene Diamine join in the aqueous solution of clay and obtain transparent pre-polymerization liquid, then pre-polymerization liquid are injected into long 40mm; Diameter is in the Glass tubing of 6mm, obtains Nanometer composite hydrogel in 48 hours 25 ℃ of following polymerizations.
(2) with 14gFeSO
47H
2O and 11.4gFe
2(SO
4)
39H
2O is dissolved in the 100g deionized water fully, and to wherein leading to N
230min is to remove O residual in the solution
2, add the 10g Nanometer composite hydrogel, soaked 72 hours down at 25 ℃.Configuration 1mol/L potassium hydroxide solution 100mL puts into the gel after the immersion, and reaction is 10 hours in closed reactor, and whole process is at N
2Carry out in the atmosphere, preparation has the Nanometer composite hydrogel of magnetic function.
Embodiment 7
(1) in the 50g deionized water, adds 5g inorganic clay Laponite XLS; After fully stirring with 10.89g vinylformic acid; 0.1g Potassium Persulphate, 0.01g Sulfothiorine join in the aqueous solution of clay and obtain transparent pre-polymerization liquid, then pre-polymerization liquid are injected into long 40mm; Diameter is in the Glass tubing of 6mm, obtains Nanometer composite hydrogel in 24 hours 25 ℃ of following polymerizations.
(2) with 7.6gFeSO
4And 10.5gFe
2(SO
4)
3Be dissolved in fully in the 100g deionized water, and to wherein leading to N
230min is to remove O residual in the solution
2, add the 10g Nanometer composite hydrogel, soaked 24 hours down at 25 ℃.Configuration 3mol/L sodium hydroxide solution 100mL puts into the gel after the immersion, and reaction is 2 hours in closed reactor, and whole process is at N
2Carry out in the atmosphere, preparation has the Nanometer composite hydrogel of magnetic function.
Claims (10)
1. preparation method with Nanometer composite hydrogel of magnetic function comprises:
(1) inorganic clay is joined in the deionized water, clay is peeled off fully, add water-soluble monomer, initiator and catalyzer then, obtain pre-polymerization liquid after mixing; The pre-polymerization liquid of gained at 5-30 ℃ of following polymerization 24-120 hour, is obtained Nanometer composite hydrogel; Wherein the massfraction of pre-polymerization liquid medium clay soil is 0.1%-20%, and the massfraction 5%-40% of water-soluble monomer, the massfraction of initiator are 0.5%-2%, and the massfraction of catalyzer is 0.0001%-0.01%, and all the other are deionized water;
(2) be dissolved in divalent iron salt and trivalent iron salt in the deionized water, add the above-mentioned Nanometer composite hydrogel of 1g-10g again, under 5-30 ℃ and nitrogen protection, soaked 24-120 hour the hydrogel after obtaining soaking;
Configuration 0.5-5mol/L coprecipitator adds the hydrogel after the above-mentioned immersion, and nitrogen protection reaction 1-12 hour down promptly gets the Nanometer composite hydrogel with magnetic function; The mol ratio of raw material is a divalent iron salt: trivalent iron salt: coprecipitator=1: 1-2.5: 1-20.
2. a kind of preparation method according to claim 1 with Nanometer composite hydrogel of magnetic function; It is characterized in that: the inorganic clay in the said step (1) is meant the inorganic lithium saponite that in water, can peel off fully; Be Laponite XLG or Laponite XLS, wherein the chemical formula of Laponite XLG is [Mg
5.34Li
0.66Si
8O
20(OH)
4] Na
0.66, LaponiteXLS is for being 92.32% [Mg by massfraction
5.34Li
0.66Si
8O
20(OH)]
4] Na
0.66With massfraction be 7.68% Na
4P
2O
7Form.
3. a kind of preparation method with Nanometer composite hydrogel of magnetic function according to claim 1 is characterized in that: the water-soluble monomer in the said step (1) is one or more in NSC 11448, vinylformic acid, the acrylic amide.
4. a kind of preparation method with Nanometer composite hydrogel of magnetic function according to claim 1 is characterized in that: the initiator in the said step (1) is one or more in Potassium Persulphate, ammonium persulphate, Sodium Persulfate, the Diisopropyl azodicarboxylate.
5. a kind of preparation method according to claim 1 with Nanometer composite hydrogel of magnetic function; It is characterized in that: the catalyzer in the said step (1) is N, N, N '; N ', one or more in-Tetramethyl Ethylene Diamine, trolamine, the Sulfothiorine.
6. a kind of preparation method with Nanometer composite hydrogel of magnetic function according to claim 1 is characterized in that: the divalent iron salt in the said step (2) is FeSO
47H
2O, FeSO
4, FeCl
2, FeCl
24H
2Among the O one or more.
7. a kind of preparation method with Nanometer composite hydrogel of magnetic function according to claim 1 is characterized in that: the ferric salt solution in the said step (2) is Fe
2(SO
4)
3, Fe
2(SO
4)
39H
2O, FeCl
3, FeCl
36H
2Among the O one or more.
8. a kind of preparation method with Nanometer composite hydrogel of magnetic function according to claim 1 is characterized in that: the coprecipitator in the said step (2) is one or more in sodium hydroxide solution, potassium hydroxide solution, the ammoniacal liquor.
9. a kind of preparation method according to claim 1 with Nanometer composite hydrogel of magnetic function; It is characterized in that: the saturation magnetization of the Nanometer composite hydrogel with magnetic function that obtains in the said step (2) is between 0.5-30emu/g, and coercive force is between 0-50Oe.
10. a kind of preparation method according to claim 1 with Nanometer composite hydrogel of magnetic function; It is characterized in that: the particle diameter of magnetic nanoparticle is between 10-100nm in the Nanometer composite hydrogel with magnetic function that obtains in the said step (2), and the massfraction of magnetic nanoparticle accounts for the 1%-30% of the hydrogel with magnetic function.
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Cited By (10)
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|---|---|---|---|---|
| CN102649954A (en) * | 2012-05-17 | 2012-08-29 | 兰州大学 | Immobilized enzyme for magnetic nanometer clay carrier and regenerating method thereof |
| CN103408683A (en) * | 2013-07-15 | 2013-11-27 | 东华大学 | Preparation method of physical/chemical crosslinking photo-thermal response hydrogel |
| CN103408708A (en) * | 2013-07-15 | 2013-11-27 | 东华大学 | Preparation method of near-infrared light response hydrogel |
| WO2015096607A1 (en) * | 2013-12-26 | 2015-07-02 | 厦门大学 | Poss-containing in situ composite nano-gel with magnetic responsiveness and preparation method therefor |
| CN105642348A (en) * | 2016-03-07 | 2016-06-08 | 湖北科技学院 | In-situ radiation preparation method of magnetic recyclable nano composite hydrogel catalytic material |
| CN107964059A (en) * | 2017-11-17 | 2018-04-27 | 合肥工业大学 | A kind of preparation method of Magnetic guidance selfreparing Nanometer composite hydrogel |
| CN107973876A (en) * | 2017-12-01 | 2018-05-01 | 东华大学 | A kind of preparation method of multiple response core-shell structure magnetic nano-hydrogel photonic crystal |
| CN108424532A (en) * | 2018-03-14 | 2018-08-21 | 西安交通大学 | A kind of preparation method of the magnetic hydrogel of high intensity high-fracture toughness |
| CN108484973A (en) * | 2018-02-05 | 2018-09-04 | 同济大学 | A method of crosslinking agent is done using barium ferrite and prepares hydrogel |
| CN110183581A (en) * | 2019-04-19 | 2019-08-30 | 武汉理工大学 | Preparation method based on the dual network structuring polymer hydrogel being physical crosslinking entirely |
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| CN102649954A (en) * | 2012-05-17 | 2012-08-29 | 兰州大学 | Immobilized enzyme for magnetic nanometer clay carrier and regenerating method thereof |
| CN103408683A (en) * | 2013-07-15 | 2013-11-27 | 东华大学 | Preparation method of physical/chemical crosslinking photo-thermal response hydrogel |
| CN103408708A (en) * | 2013-07-15 | 2013-11-27 | 东华大学 | Preparation method of near-infrared light response hydrogel |
| CN103408708B (en) * | 2013-07-15 | 2017-02-08 | 东华大学 | Preparation method of near-infrared light response hydrogel |
| WO2015096607A1 (en) * | 2013-12-26 | 2015-07-02 | 厦门大学 | Poss-containing in situ composite nano-gel with magnetic responsiveness and preparation method therefor |
| CN105642348A (en) * | 2016-03-07 | 2016-06-08 | 湖北科技学院 | In-situ radiation preparation method of magnetic recyclable nano composite hydrogel catalytic material |
| CN107964059A (en) * | 2017-11-17 | 2018-04-27 | 合肥工业大学 | A kind of preparation method of Magnetic guidance selfreparing Nanometer composite hydrogel |
| CN107964059B (en) * | 2017-11-17 | 2019-08-30 | 合肥工业大学 | A kind of preparation method of Magnetic guidance selfreparing Nanometer composite hydrogel |
| CN107973876A (en) * | 2017-12-01 | 2018-05-01 | 东华大学 | A kind of preparation method of multiple response core-shell structure magnetic nano-hydrogel photonic crystal |
| CN107973876B (en) * | 2017-12-01 | 2021-03-19 | 东华大学 | Preparation method of magnetic nano hydrogel photonic crystal with multi-responsiveness core-shell structure |
| CN108484973A (en) * | 2018-02-05 | 2018-09-04 | 同济大学 | A method of crosslinking agent is done using barium ferrite and prepares hydrogel |
| CN108424532A (en) * | 2018-03-14 | 2018-08-21 | 西安交通大学 | A kind of preparation method of the magnetic hydrogel of high intensity high-fracture toughness |
| CN108424532B (en) * | 2018-03-14 | 2020-05-15 | 西安交通大学 | Preparation method of magnetic hydrogel with high strength and high fracture toughness |
| CN110183581A (en) * | 2019-04-19 | 2019-08-30 | 武汉理工大学 | Preparation method based on the dual network structuring polymer hydrogel being physical crosslinking entirely |
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